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This document summarizes guidelines for validating analytical methods as outlined by the International Council for Harmonisation (ICH). It discusses key aspects of method validation that should be considered, including specificity, linearity, range, accuracy, precision, detection limit, quantitation limit, robustness, and ruggedness. Specific procedures for establishing each parameter are provided. The objective of validation is to demonstrate that the analytical method is suitable for its intended purpose by consistently producing reliable results. Validation helps ensure the quality, safety, and efficacy of pharmaceutical products.
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Validation of analytical methods
Analytical methods plays a vital role in new drug development, Preformulation and formulation studies, stability studies and quality control testing.
Method validation
This document outlines the key steps in method validation for clinical chemistry laboratories. It defines method validation and discusses when methods should be validated. The key aspects that must be validated include calibration, precision, accuracy, linearity, limit of detection, analytical range, sensitivity, specificity, ruggedness and robustness. Thorough documentation of the validation study is also required. Validating a method involves experimentally testing these parameters and documenting the results to provide objective evidence that the method is suitable for its intended use.
Analytical method validation
This document provides an overview of analytical method validation. It discusses key validation characteristics such as specificity, linearity, range, accuracy, precision, LOD and LOQ. Guidelines for validation from organizations like ICH, USP, ANVISA and AOAC are also mentioned. The document describes procedures for establishing various validation parameters and evaluating the results. It emphasizes that validation is necessary to ensure analytical methods consistently provide reliable results.
Method Validation - ICH /USP Validation, Linearity and Repeatability
1. The document provides an overview of method validation requirements from various regulatory bodies and guidelines. It discusses key validation parameters such as specificity, linearity, range, accuracy, precision, detection limit, and quantitation limit.
2. Validation is required to demonstrate that analytical methods are suitable for their intended purposes. It identifies potential sources of error and quantifies errors in the method. Validation includes parameters like linearity, range, accuracy, and precision.
3. The document provides details on establishing various validation parameters according to regulatory guidelines from ICH, FDA, and USP. It also discusses considerations for validating methods like instrument qualification and defines method life cycles.
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Analytical method validation is important for new drug development, formulation studies, stability studies, and quality control testing. Validation ensures a method is simple, specific, accurate, precise, economical, and convenient. It provides high assurance that a process will consistently produce quality products meeting specifications. Analytical validation evaluates a method's suitability for its intended purpose by assessing accuracy, precision, specificity, linearity, range, detection limit, quantitation limit, robustness, ruggedness, sensitivity, repeatability, and reproducibility.
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This document discusses the key aspects of analytical method validation including specificity, linearity, range, accuracy, precision, detection limit, quantitation limit, robustness, and system suitability testing. It provides detailed descriptions and recommendations for establishing each validation characteristic to demonstrate that an analytical procedure is suitable for its intended use.
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This document discusses validation of analytical procedures for drug substances and products. It describes key validation characteristics including specificity, accuracy, precision (repeatability and intermediate precision), detection limit, quantitation limit, linearity, range, and robustness. Validation is required for identification tests, assays of active ingredients and selected components, and tests for impurities. The level of validation depends on the objective and type of analytical procedure.
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Validation of analytical methods
Analytical methods plays a vital role in new drug development, Preformulation and formulation studies, stability studies and quality control testing.
Method validation
This document outlines the key steps in method validation for clinical chemistry laboratories. It defines method validation and discusses when methods should be validated. The key aspects that must be validated include calibration, precision, accuracy, linearity, limit of detection, analytical range, sensitivity, specificity, ruggedness and robustness. Thorough documentation of the validation study is also required. Validating a method involves experimentally testing these parameters and documenting the results to provide objective evidence that the method is suitable for its intended use.
Analytical method validation
This document provides an overview of analytical method validation. It discusses key validation characteristics such as specificity, linearity, range, accuracy, precision, LOD and LOQ. Guidelines for validation from organizations like ICH, USP, ANVISA and AOAC are also mentioned. The document describes procedures for establishing various validation parameters and evaluating the results. It emphasizes that validation is necessary to ensure analytical methods consistently provide reliable results.
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1. The document provides an overview of method validation requirements from various regulatory bodies and guidelines. It discusses key validation parameters such as specificity, linearity, range, accuracy, precision, detection limit, and quantitation limit.
2. Validation is required to demonstrate that analytical methods are suitable for their intended purposes. It identifies potential sources of error and quantifies errors in the method. Validation includes parameters like linearity, range, accuracy, and precision.
3. The document provides details on establishing various validation parameters according to regulatory guidelines from ICH, FDA, and USP. It also discusses considerations for validating methods like instrument qualification and defines method life cycles.
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Analytical method validation is important for new drug development, formulation studies, stability studies, and quality control testing. Validation ensures a method is simple, specific, accurate, precise, economical, and convenient. It provides high assurance that a process will consistently produce quality products meeting specifications. Analytical validation evaluates a method's suitability for its intended purpose by assessing accuracy, precision, specificity, linearity, range, detection limit, quantitation limit, robustness, ruggedness, sensitivity, repeatability, and reproducibility.
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This document discusses the key aspects of analytical method validation including specificity, linearity, range, accuracy, precision, detection limit, quantitation limit, robustness, and system suitability testing. It provides detailed descriptions and recommendations for establishing each validation characteristic to demonstrate that an analytical procedure is suitable for its intended use.
Analytical method validation
This document discusses validation in the pharmaceutical industry. It begins by defining validation as establishing evidence that a process maintains compliance. It then discusses why validation is important, including that regulatory agencies require validation to ensure consistent, reproducible results. It outlines the types of validation including equipment, facilities, analytical methods, and more. It focuses on analytical method validation, discussing parameters like accuracy, precision, specificity, and more. It emphasizes that validation is necessary to confirm analytical procedures consistently produce the intended results.
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This document discusses validation of analytical procedures for drug substances and products. It describes key validation characteristics including specificity, accuracy, precision (repeatability and intermediate precision), detection limit, quantitation limit, linearity, range, and robustness. Validation is required for identification tests, assays of active ingredients and selected components, and tests for impurities. The level of validation depends on the objective and type of analytical procedure.
Analytical Method Validation as per ICH vs USP
How analytical method validation differs between ICH and USP.
Includes basis definition and difference.
Method Validation: What Are Its Key Parameters
What is Validation?
Methods validation is the process of demonstrating that analytical procedures are suitable for their intended use-Guidance for Industry
Validation is a process-risk will determine the effort
High Risk:Total validation
Moderate Risk:Testing,Documentation
Low Risk:Testing the change
Accuracy
ICH defines accuracy of an analytical procedure as the closeness of agreement between the conventional true value or an accepted reference value and the value found.
% Accuracy = Experimental- True Value * 100
True Value
Precision
Precision of analytical procedure is defined as closeness of agreement in values between a series of measurements. As per ICH, precision is considered at three different levels:
Repeatability or intra—assay precision: precision data are obtained by repeatedly analyzing, in one lab on one day, aliquots of a homogeneous sample.
Intermediate precision: precision obtained when the assay is performed by multiple analysts, multiple instruments, and multiple days in one lab.
Reproducibility: precision between laboratories.
Specificity
Specificity is the ability of the method to accurately measure the analyte response in the presence of all potential sample components.
It is very important in the analysis of complex mixtures by GC, HPLC, AA, ICP, etc.
Limit of Detection (LOD)
Limit of Detection (LOD) is the lowest amount of analyte in a sample which can be reliably detected but not necessarily accurately or precisely measured.
Signal/Noise = 2 to 3
Limit of Quantitation (LOQ)
Limit of Quantitation (LOQ) is the lowest amount of an analyte that can be quantitatively determined with suitable precision and accuracy.
Signal/Noise = 10 to 20
Linearity and Range
Linearity of an analytical procedure is its ability (within a given range) to obtain test results which are directly proportional to the concentration (amount) of analyte in the sample.
Range: Interval from the upper to the lower concentration (amounts) of analyte in the sample (including these concentrations) for which it has been demonstrated that the analytical procedure has a suitable level of precision, accuracy and linearity
Must cover 80-120% of product claims
Usually evaluated from the same data set as linearity, precision, accuracy
Want to learn more about analytical method validation, FDA requirements and best practices to comply with them? ComplianceOnline webinars and seminars are a great training resource. Check out the following links:
ICH, FDA and USP Requirements for Method Validation
How to Validate Analytical Methods and Procedures
Validation of Analytical Methods and Procedures
Eliminate the Confusion - Analytical Method Qualification and Validation
Lifecycle Approach to Analytical Methods with QbD Elements
Analytical Instrument Qualification and System Validation
Lifecycle Approach to Analytical Methods for Drug Products
For details vis
Analytical method validation
This document discusses various concepts related to analytical method validation including accuracy, precision, specificity, detection limit, and quantitation limit. It provides definitions and recommendations for determining each concept. For accuracy, it recommends assessing using spiked samples or an independent procedure and reporting as percent recovery. For precision, it recommends determining repeatability using 9 determinations at 3 concentrations and reporting as standard deviation and coefficient of variation. Detection limit can be determined visually, by signal-to-noise ratio, or by standard deviation of the blank. Quantitation limit is the lowest concentration that can be quantified and can also be determined visually or by signal-to-noise ratio.
Analytical methods validation as per ich & usp
This document discusses analytical method validation as per ICH and USP guidelines. It defines validation as establishing documentary evidence that a procedure maintains compliance. Method validation involves demonstrating that an analytical procedure is suitable for its intended purpose by testing parameters such as accuracy, precision, specificity, detection limit, quantitation limit, linearity, range, ruggedness and robustness. It also discusses the different types of analytical procedures that require validation including identification tests, quantitative impurity tests, limit tests and assays.
analytical method validation
This document discusses analytical method validation. It provides guidance on validation from various organizations. It describes the types of analytical procedures that require validation including chromatographic, spectroscopic, and dissolution methods. Key validation characteristics that should be considered include specificity, linearity, range, accuracy, precision, detection limit, quantitation limit, robustness, and system suitability. The document provides details on how these characteristics should be determined during the validation process. It also discusses circumstances under which revalidation may be necessary such as changes to the drug synthesis or analytical method.
Analytical method validation 2020
This document provides a summary of analytical method validation. It discusses the types of analytical procedures that should be validated, including identification tests, quantitative impurity tests, limit tests, and active moiety assays. It also summarizes key validation characteristics that should be considered, such as accuracy, precision, specificity, range, detection limit, quantitation limit, linearity, and robustness. The document provides definitions and methodology recommendations for validating analytical procedures. It emphasizes that the validation process verifies that an analytical method is suitable for its intended purpose.
Method validation for drug substances and drug product _remodified_2014
Method validation is the process of proving that an analytical method is acceptable for its intended purposes.
METHOD VALIDATION = ERROR ASSESSMENT
Method validation is the process of demonstrating that analytical procedures are suitable for their intended use and that they support the identity, strength, quality, purity and potency of the drug substances and drug products
Validation: Prior Considerations Suitability of Instrument Status of Qualification and Calibration Suitability of Materials Status of Reference Standards, Reagents, Placebo Lots Suitability of Analyst Status of Training and Qualification Records Suitability of Documentation Written and approved standard test procedure and proper approved protocol with pre-established acceptance criteria
Compendial vs. Non-compendial Methods
Compendial methods-Verification
Regulatory analytical procedure in USP/NF
Non- compendial methods-Validation
Alternative analytical procedure proposed by the applicant for use instead of the regulatory analytical procedure
Chromatographic Methods
Demonstrate Resolution
Impurities/Degradants Available
Spike with impurities/degradants
Show resolution and a lack of interference
Impurities/Degradants Not Available
Stress SamplesFor assay, Stressed and Unstressed Samples should be compared.
Ability of an analytical method to measure the analyte free from interference due to other components.
Selectivity describes the ability of an analytical method to differentiate various substances in a sample
Original term used in USP
Also Preferred by IUPAC and AOAC
Also used to characterize chromatographic columns
Degree of Bias (Used in USP)
The difference in assay results between the two groups
the sample containing added impurities, degradation products, related chemical compounds, placebo ingredients
Selectivity: For impurity test, impurity profiles should be compared.
Temperature (50-60℃)
Humidity (70-80%)
Acid Hydrolysis (0.1 N HCl)
Base Hydrolysis (0.1 N NaOH)
Oxidation (3-30%)
Light (UV/Vis/Fl)
Intent is to create 10 to 30 % Degradation
Change in the analytical procedure, drug substance, drug product, the changes, may necessitate revalidation of the analytical procedures.
“The degree of revalidation depends on the nature of the change.”
“FDA intends to provide guidance in the future on post-approval changes in analytical procedures.”
By Visual Inspection of plot of signals vs. analyte concentration
By Appropriate statistical methods
Linear Regression (y = mx + b)
Correlation Coefficient, y-intercept (b), slope (m)
Acceptance criteria: Linear regression r2 > 0.999
Requires a minimum of 6 concentration levels
Normally derived from Linearity studies.
Established by confirming that the method provides acceptable degree of linearity, accuracy, and precision.
Specific range dependent upon intended application of the procedure.
Analytical method validation
This presentation was made to solely for students to make them aware/ understand basics of “Analytical Method Validation”. These slides are part of lectures delivered in M. Pharmacy Curriculum & taken up from various books and websites
A Step-by-Step Guide for Method Validation
What is Validation?
Methods validation is the process of demonstrating that analytical procedures are suitable for their intended use-Guidance for Industry
Validation is a process-risk will determine the effort
High Risk:Total validation
Moderate Risk:Testing,Documentation
Low Risk:Testing the change
Validation of Analytical Methods-Key Steps
Preparation
Experimentation
Transfering Method
Documentation
Step 1- Preparation
Develop validation project plan
Define purpose/scope of method (performance criteria)
Define and verify performance of equipment
Qualify/validate materials
Qualify/train operator
Step 2- Experimentation
Perform validation experiments- may have to change either equipment or limits
Develop SOPs for executing the method in routine
Define type and frequency of system suitability tests and/or analytical quality control (AQC) checks
Define change control procedure
Document validation experiments and results
Step 3- Transferring Methods to Routine Laboratories
Designate project owner
Develop procedure on how to use method
Develop system suitability tests (test procedure, frequency, acceptance criteria)
Define transfer tests and acceptance criteria in the routine
Train routine lab analyst in development lab
Repeat 2 critical method validation tests in routine lab
Analyze at least three samples in development and routine lab
Analyst in routine lab should give frequent feedback
Step 4- Documentation for the FDA
Validation report and supporting documentation:
Objective, scope
Methodology
Materials
Equipment
Validation data
Supporting documentation (chromatograms, spectra)
Transfer to routine protocol
Reference to SOP
Want to learn more about analytical method validation, FDA and ICH requirements and best practices to comply with them? ComplianceOnline webinars and seminars are a great training resource. Check out the following links:
ICH, FDA and USP Requirements for Method Validation
How to Validate Analytical Methods and Procedures
Validation of Analytical Methods and Procedures
Eliminate the Confusion - Analytical Method Qualification and Validation
Lifecycle Approach to Analytical Methods with QbD Elements
Analytical Instrument Qualification and System Validation
Lifecycle Approach to Analytical Methods for Drug Products
For more details:http://www.complianceonline.com/validation-of-analytical-methods-and-procedures-webinar-training-701615-prdw?channel=valppt
Sampling analysis-reporting
The document discusses the key steps in a laboratory process for sampling, analyzing samples, and reporting results. It covers technical requirements for sampling and analysis, selecting suitable analytical procedures, maintaining quality assurance, and describing the flow from receiving samples to issuing a report. Critical aspects like equipment calibration, method validation, quality control, and estimating measurement uncertainty are emphasized.
Analytical Method Validation
This document discusses analytical method validation. It provides definitions and guidelines for validating analytical methods from regulatory agencies. Key aspects of method validation discussed include accuracy, precision, specificity, range, linearity, limits of detection and quantification. Validation parameters are described for different types of analytical tests including identification, quantitative impurity tests and assays. Guidelines are provided for qualifying analytical instrumentation and categorizing instruments based on complexity.
Analytical method validation by manoj ingale(best ppts)
here you will get every aspect and detailed information about the validation of analytical methods.hope it will give u the all information u required.
Q2 r1 guidelines
The document discusses validation of analytical procedures. It defines validation as establishing by laboratory studies that an analytical procedure meets requirements for its intended use. It describes the typical steps in validating identification tests, quantitative impurity tests, and assays. Key validation characteristics discussed include specificity, linearity, range, accuracy, precision, detection and quantitation limits, robustness, and ruggedness. The guidelines provide details on establishing each characteristic to help ensure analytical methods are suitable for their intended pharmaceutical applications.
Validation of qualitative lab test methods
this lecture describes the methods used and recommended by CLSI to validate both the qualitative and semi-Quantitative laboratory test methods
Analytical Method Validation basics by Dr. A. Amsavel
This document discusses analytical method validation which is the process of confirming that an analytical method is suitable for its intended purpose. Key aspects of method validation discussed include accuracy, precision, specificity, linearity, range, detection limit, quantitation limit, repeatability and intermediate precision. The document outlines validation parameters for different types of analytical methods and provides examples of acceptance criteria. It also discusses guidance from regulatory agencies on analytical method validation.
Analytical method validation
This document discusses guidelines for analytical method validation. It outlines the types of analytical methods that require validation including chromatographic, spectroscopic, and dissolution methods. It describes key performance characteristics that are evaluated in validation studies such as specificity, accuracy, precision, linearity, range, detection and quantitation limits, and robustness. The document provides details on how these characteristics are tested and the acceptance criteria used to ensure the method is suitable for its intended purpose. It also discusses circumstances under which revalidation may be necessary.
ICH-Q2 AMV
This document discusses validation of analytical procedures. It is divided into two parts. Part I provides definitions and discusses typical validation characteristics such as accuracy, precision, specificity, detection limit, and quantitation limit. Part II provides more detailed methodology guidance on how to validate these characteristics. It describes how to validate specificity, accuracy, precision, detection limit, quantitation limit, linearity, range, and robustness of analytical procedures. The goal of validation is to demonstrate that analytical procedures are suitable for their intended purpose in identifying, quantifying, and testing impurities in drug substances and products.
ANALYTICAL METHOD VALIDATION -A PREDICAMENT OF SERVICE PROVIDER
This document discusses analytical method validation and outlines the challenges faced when outsourcing these services. It notes that while full validation according to ICH guidelines may not always be necessary, methods should still be scientifically sound. Some ways to reduce validation efforts discussed include adjusting the scope based on development stage, establishing method feasibility early on, and employing a risk-based approach. The responsibilities of both service providers and sponsors are examined, with the importance of alignment on quality expectations through a detailed agreement emphasized.
Analytical Method Validation
This document outlines guidelines for analytical method validation as described in ICH Q2. It defines validation as establishing evidence that a method is suitable for its intended purpose. Key parameters that must be validated include accuracy, precision, specificity, detection limit, quantitation limit, linearity, range, and robustness. The guidelines provide details on how to validate these parameters and determine method suitability.
Analytical method validation
This document summarizes guidelines for analytical method validation from various regulatory agencies. It discusses the purpose of validation to verify method suitability for submissions. Key validation characteristics covered include specificity, linearity, range, accuracy, precision, detection/quantitation limits, robustness, and system suitability testing. It notes that revalidation may be necessary if the analytical method or drug product is changed.
Analytical method validation as per ich and usp
Analytical method validation is a process of documenting/ proving that an analytical method provides analytical data acceptable for the intended use.After the development of an analytical procedure, it is must important to assure that the procedure will consistently produce the intended a precise result with high degree of accuracy. The method should give a specific result that may not be affected by external matters. This creates a requirement to validate the analytical procedures. The validation procedures consists of some characteristics parameters that makes the method acceptable with addition of statistical tools.
Phase Appropriate Method Validation Aryo Boston-Nitto 2
The document discusses phase appropriate method validation. It provides guidelines for validating analytical methods based on the intended use and stage of product development. Validation requirements become more extensive in later phases, from proof of concept in Phase I to full validation in Phase III. Key validation characteristics discussed include specificity, selectivity, range, accuracy, precision, detection limit, quantitation limit, linearity and robustness. The document also covers stress studies, system suitability criteria, and the differences between stability indicating and specificity methods.
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Analytical Method Validation as per ICH vs USP
How analytical method validation differs between ICH and USP.
Includes basis definition and difference.
Method Validation: What Are Its Key Parameters
What is Validation?
Methods validation is the process of demonstrating that analytical procedures are suitable for their intended use-Guidance for Industry
Validation is a process-risk will determine the effort
High Risk:Total validation
Moderate Risk:Testing,Documentation
Low Risk:Testing the change
Accuracy
ICH defines accuracy of an analytical procedure as the closeness of agreement between the conventional true value or an accepted reference value and the value found.
% Accuracy = Experimental- True Value * 100
True Value
Precision
Precision of analytical procedure is defined as closeness of agreement in values between a series of measurements. As per ICH, precision is considered at three different levels:
Repeatability or intra—assay precision: precision data are obtained by repeatedly analyzing, in one lab on one day, aliquots of a homogeneous sample.
Intermediate precision: precision obtained when the assay is performed by multiple analysts, multiple instruments, and multiple days in one lab.
Reproducibility: precision between laboratories.
Specificity
Specificity is the ability of the method to accurately measure the analyte response in the presence of all potential sample components.
It is very important in the analysis of complex mixtures by GC, HPLC, AA, ICP, etc.
Limit of Detection (LOD)
Limit of Detection (LOD) is the lowest amount of analyte in a sample which can be reliably detected but not necessarily accurately or precisely measured.
Signal/Noise = 2 to 3
Limit of Quantitation (LOQ)
Limit of Quantitation (LOQ) is the lowest amount of an analyte that can be quantitatively determined with suitable precision and accuracy.
Signal/Noise = 10 to 20
Linearity and Range
Linearity of an analytical procedure is its ability (within a given range) to obtain test results which are directly proportional to the concentration (amount) of analyte in the sample.
Range: Interval from the upper to the lower concentration (amounts) of analyte in the sample (including these concentrations) for which it has been demonstrated that the analytical procedure has a suitable level of precision, accuracy and linearity
Must cover 80-120% of product claims
Usually evaluated from the same data set as linearity, precision, accuracy
Want to learn more about analytical method validation, FDA requirements and best practices to comply with them? ComplianceOnline webinars and seminars are a great training resource. Check out the following links:
ICH, FDA and USP Requirements for Method Validation
How to Validate Analytical Methods and Procedures
Validation of Analytical Methods and Procedures
Eliminate the Confusion - Analytical Method Qualification and Validation
Lifecycle Approach to Analytical Methods with QbD Elements
Analytical Instrument Qualification and System Validation
Lifecycle Approach to Analytical Methods for Drug Products
For details vis
Analytical method validation
This document discusses various concepts related to analytical method validation including accuracy, precision, specificity, detection limit, and quantitation limit. It provides definitions and recommendations for determining each concept. For accuracy, it recommends assessing using spiked samples or an independent procedure and reporting as percent recovery. For precision, it recommends determining repeatability using 9 determinations at 3 concentrations and reporting as standard deviation and coefficient of variation. Detection limit can be determined visually, by signal-to-noise ratio, or by standard deviation of the blank. Quantitation limit is the lowest concentration that can be quantified and can also be determined visually or by signal-to-noise ratio.
Analytical methods validation as per ich & usp
This document discusses analytical method validation as per ICH and USP guidelines. It defines validation as establishing documentary evidence that a procedure maintains compliance. Method validation involves demonstrating that an analytical procedure is suitable for its intended purpose by testing parameters such as accuracy, precision, specificity, detection limit, quantitation limit, linearity, range, ruggedness and robustness. It also discusses the different types of analytical procedures that require validation including identification tests, quantitative impurity tests, limit tests and assays.
analytical method validation
This document discusses analytical method validation. It provides guidance on validation from various organizations. It describes the types of analytical procedures that require validation including chromatographic, spectroscopic, and dissolution methods. Key validation characteristics that should be considered include specificity, linearity, range, accuracy, precision, detection limit, quantitation limit, robustness, and system suitability. The document provides details on how these characteristics should be determined during the validation process. It also discusses circumstances under which revalidation may be necessary such as changes to the drug synthesis or analytical method.
Analytical method validation 2020
This document provides a summary of analytical method validation. It discusses the types of analytical procedures that should be validated, including identification tests, quantitative impurity tests, limit tests, and active moiety assays. It also summarizes key validation characteristics that should be considered, such as accuracy, precision, specificity, range, detection limit, quantitation limit, linearity, and robustness. The document provides definitions and methodology recommendations for validating analytical procedures. It emphasizes that the validation process verifies that an analytical method is suitable for its intended purpose.
Method validation for drug substances and drug product _remodified_2014
Method validation is the process of proving that an analytical method is acceptable for its intended purposes.
METHOD VALIDATION = ERROR ASSESSMENT
Method validation is the process of demonstrating that analytical procedures are suitable for their intended use and that they support the identity, strength, quality, purity and potency of the drug substances and drug products
Validation: Prior Considerations Suitability of Instrument Status of Qualification and Calibration Suitability of Materials Status of Reference Standards, Reagents, Placebo Lots Suitability of Analyst Status of Training and Qualification Records Suitability of Documentation Written and approved standard test procedure and proper approved protocol with pre-established acceptance criteria
Compendial vs. Non-compendial Methods
Compendial methods-Verification
Regulatory analytical procedure in USP/NF
Non- compendial methods-Validation
Alternative analytical procedure proposed by the applicant for use instead of the regulatory analytical procedure
Chromatographic Methods
Demonstrate Resolution
Impurities/Degradants Available
Spike with impurities/degradants
Show resolution and a lack of interference
Impurities/Degradants Not Available
Stress SamplesFor assay, Stressed and Unstressed Samples should be compared.
Ability of an analytical method to measure the analyte free from interference due to other components.
Selectivity describes the ability of an analytical method to differentiate various substances in a sample
Original term used in USP
Also Preferred by IUPAC and AOAC
Also used to characterize chromatographic columns
Degree of Bias (Used in USP)
The difference in assay results between the two groups
the sample containing added impurities, degradation products, related chemical compounds, placebo ingredients
Selectivity: For impurity test, impurity profiles should be compared.
Temperature (50-60℃)
Humidity (70-80%)
Acid Hydrolysis (0.1 N HCl)
Base Hydrolysis (0.1 N NaOH)
Oxidation (3-30%)
Light (UV/Vis/Fl)
Intent is to create 10 to 30 % Degradation
Change in the analytical procedure, drug substance, drug product, the changes, may necessitate revalidation of the analytical procedures.
“The degree of revalidation depends on the nature of the change.”
“FDA intends to provide guidance in the future on post-approval changes in analytical procedures.”
By Visual Inspection of plot of signals vs. analyte concentration
By Appropriate statistical methods
Linear Regression (y = mx + b)
Correlation Coefficient, y-intercept (b), slope (m)
Acceptance criteria: Linear regression r2 > 0.999
Requires a minimum of 6 concentration levels
Normally derived from Linearity studies.
Established by confirming that the method provides acceptable degree of linearity, accuracy, and precision.
Specific range dependent upon intended application of the procedure.
Analytical method validation
This presentation was made to solely for students to make them aware/ understand basics of “Analytical Method Validation”. These slides are part of lectures delivered in M. Pharmacy Curriculum & taken up from various books and websites
A Step-by-Step Guide for Method Validation
What is Validation?
Methods validation is the process of demonstrating that analytical procedures are suitable for their intended use-Guidance for Industry
Validation is a process-risk will determine the effort
High Risk:Total validation
Moderate Risk:Testing,Documentation
Low Risk:Testing the change
Validation of Analytical Methods-Key Steps
Preparation
Experimentation
Transfering Method
Documentation
Step 1- Preparation
Develop validation project plan
Define purpose/scope of method (performance criteria)
Define and verify performance of equipment
Qualify/validate materials
Qualify/train operator
Step 2- Experimentation
Perform validation experiments- may have to change either equipment or limits
Develop SOPs for executing the method in routine
Define type and frequency of system suitability tests and/or analytical quality control (AQC) checks
Define change control procedure
Document validation experiments and results
Step 3- Transferring Methods to Routine Laboratories
Designate project owner
Develop procedure on how to use method
Develop system suitability tests (test procedure, frequency, acceptance criteria)
Define transfer tests and acceptance criteria in the routine
Train routine lab analyst in development lab
Repeat 2 critical method validation tests in routine lab
Analyze at least three samples in development and routine lab
Analyst in routine lab should give frequent feedback
Step 4- Documentation for the FDA
Validation report and supporting documentation:
Objective, scope
Methodology
Materials
Equipment
Validation data
Supporting documentation (chromatograms, spectra)
Transfer to routine protocol
Reference to SOP
Want to learn more about analytical method validation, FDA and ICH requirements and best practices to comply with them? ComplianceOnline webinars and seminars are a great training resource. Check out the following links:
ICH, FDA and USP Requirements for Method Validation
How to Validate Analytical Methods and Procedures
Validation of Analytical Methods and Procedures
Eliminate the Confusion - Analytical Method Qualification and Validation
Lifecycle Approach to Analytical Methods with QbD Elements
Analytical Instrument Qualification and System Validation
Lifecycle Approach to Analytical Methods for Drug Products
For more details:http://www.complianceonline.com/validation-of-analytical-methods-and-procedures-webinar-training-701615-prdw?channel=valppt
Sampling analysis-reporting
The document discusses the key steps in a laboratory process for sampling, analyzing samples, and reporting results. It covers technical requirements for sampling and analysis, selecting suitable analytical procedures, maintaining quality assurance, and describing the flow from receiving samples to issuing a report. Critical aspects like equipment calibration, method validation, quality control, and estimating measurement uncertainty are emphasized.
Analytical Method Validation
This document discusses analytical method validation. It provides definitions and guidelines for validating analytical methods from regulatory agencies. Key aspects of method validation discussed include accuracy, precision, specificity, range, linearity, limits of detection and quantification. Validation parameters are described for different types of analytical tests including identification, quantitative impurity tests and assays. Guidelines are provided for qualifying analytical instrumentation and categorizing instruments based on complexity.
Analytical method validation by manoj ingale(best ppts)
here you will get every aspect and detailed information about the validation of analytical methods.hope it will give u the all information u required.
Q2 r1 guidelines
The document discusses validation of analytical procedures. It defines validation as establishing by laboratory studies that an analytical procedure meets requirements for its intended use. It describes the typical steps in validating identification tests, quantitative impurity tests, and assays. Key validation characteristics discussed include specificity, linearity, range, accuracy, precision, detection and quantitation limits, robustness, and ruggedness. The guidelines provide details on establishing each characteristic to help ensure analytical methods are suitable for their intended pharmaceutical applications.
Validation of qualitative lab test methods
this lecture describes the methods used and recommended by CLSI to validate both the qualitative and semi-Quantitative laboratory test methods
Analytical Method Validation basics by Dr. A. Amsavel
This document discusses analytical method validation which is the process of confirming that an analytical method is suitable for its intended purpose. Key aspects of method validation discussed include accuracy, precision, specificity, linearity, range, detection limit, quantitation limit, repeatability and intermediate precision. The document outlines validation parameters for different types of analytical methods and provides examples of acceptance criteria. It also discusses guidance from regulatory agencies on analytical method validation.
Analytical method validation
This document discusses guidelines for analytical method validation. It outlines the types of analytical methods that require validation including chromatographic, spectroscopic, and dissolution methods. It describes key performance characteristics that are evaluated in validation studies such as specificity, accuracy, precision, linearity, range, detection and quantitation limits, and robustness. The document provides details on how these characteristics are tested and the acceptance criteria used to ensure the method is suitable for its intended purpose. It also discusses circumstances under which revalidation may be necessary.
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This document discusses validation of analytical procedures. It is divided into two parts. Part I provides definitions and discusses typical validation characteristics such as accuracy, precision, specificity, detection limit, and quantitation limit. Part II provides more detailed methodology guidance on how to validate these characteristics. It describes how to validate specificity, accuracy, precision, detection limit, quantitation limit, linearity, range, and robustness of analytical procedures. The goal of validation is to demonstrate that analytical procedures are suitable for their intended purpose in identifying, quantifying, and testing impurities in drug substances and products.
ANALYTICAL METHOD VALIDATION -A PREDICAMENT OF SERVICE PROVIDER
This document discusses analytical method validation and outlines the challenges faced when outsourcing these services. It notes that while full validation according to ICH guidelines may not always be necessary, methods should still be scientifically sound. Some ways to reduce validation efforts discussed include adjusting the scope based on development stage, establishing method feasibility early on, and employing a risk-based approach. The responsibilities of both service providers and sponsors are examined, with the importance of alignment on quality expectations through a detailed agreement emphasized.
Analytical Method Validation
This document outlines guidelines for analytical method validation as described in ICH Q2. It defines validation as establishing evidence that a method is suitable for its intended purpose. Key parameters that must be validated include accuracy, precision, specificity, detection limit, quantitation limit, linearity, range, and robustness. The guidelines provide details on how to validate these parameters and determine method suitability.
Analytical method validation
This document summarizes guidelines for analytical method validation from various regulatory agencies. It discusses the purpose of validation to verify method suitability for submissions. Key validation characteristics covered include specificity, linearity, range, accuracy, precision, detection/quantitation limits, robustness, and system suitability testing. It notes that revalidation may be necessary if the analytical method or drug product is changed.
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Analytical method validation is a process of documenting/ proving that an analytical method provides analytical data acceptable for the intended use.After the development of an analytical procedure, it is must important to assure that the procedure will consistently produce the intended a precise result with high degree of accuracy. The method should give a specific result that may not be affected by external matters. This creates a requirement to validate the analytical procedures. The validation procedures consists of some characteristics parameters that makes the method acceptable with addition of statistical tools.
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This document summarizes guidelines for analytical method validation from various regulatory agencies. It discusses the purpose of validation to verify method suitability. Key analytical performance characteristics covered include specificity, linearity, range, accuracy, precision, detection/quantitation limits, robustness, and system suitability testing. It notes that revalidation may be necessary if the analytical method or drug product is changed.
ICH and WHO Guideline for Validation and Calibration.pptx
Validation: Action of proving and documenting that any process, procedure or method actually and consistently leads to the expected results.
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This presentation summarizes ICH and WHO guidelines for validation and calibration of equipment. It discusses the key aspects of validation including design qualification, installation qualification, operational qualification, and performance qualification. Validation ensures a process or method consistently produces the expected results. Calibration establishes the relationship between instrument readings and known standard values. The presentation also outlines validation characteristics like specificity, accuracy, precision according to ICH guidelines. Overall, the presentation provides a concise overview of important concepts and steps for validating analytical equipment and methods.
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This document discusses guidelines for analytical method validation. It outlines types of analytical methods that require validation including chromatographic, spectroscopic, and dissolution methods. Key analytical performance characteristics used in validation are described such as specificity, linearity, range, accuracy, precision, detection/quantitation limits, robustness, and system suitability testing. The document provides details on determining these characteristics and validating methods. It also addresses revalidation and references for further information.
Analytical method validation
This document discusses analytical method validation. It defines analytical method validation as providing assurance that an analytical method can consistently and accurately determine the presence or quantity of attributes. The objectives of validation are to obtain consistent, reliable and accurate data. Key parameters that are assessed in validation include specificity, accuracy, precision, linearity, range, limits of detection and quantification, ruggedness and robustness. The validation process involves planning, testing method performance characteristics, selecting validation acceptance criteria, and documenting results in a validation report. Validation is important for analytical methods used in pharmaceutical analysis.
Validation
This document discusses validation in the pharmaceutical industry. It defines validation as confirming that a process, procedure, or system achieves the desired results. There are various types of validation including process, equipment, facility, analytical method, and computer system validation. Process validation involves establishing scientific evidence that a process is capable of consistently producing quality products. The key stages of process validation are process design, process qualification, and continued process verification. Common validation parameters discussed include accuracy, precision, specificity, linearity, range, limit of detection, limit of quantification, ruggedness, and robustness.
Analytical method validation
The document discusses analytical method validation. It defines validation as establishing evidence that a process will consistently produce a product meeting predetermined specifications. The objectives are to discuss aspects of validation including principles, approaches, and characteristics. Key steps in validation are establishing accuracy, precision, specificity, linearity, range, limits of detection and quantification, and robustness of analytical procedures used for identification, quantification of impurities and active ingredients.
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The document discusses process validation in the pharmaceutical industry. It defines process validation as ensuring a manufacturing process is capable of consistently producing a product meeting its predetermined specifications and quality attributes. The summary describes the three stages of process validation: process design, process qualification, and continued process verification. Key parameters that must be validated for analytical methods used in process validation are also listed, including specificity, linearity, accuracy, precision, limits of detection and quantification, and heat sensitivity.
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The document discusses analytical method validation which is required by pharmaceutical GMPs. It defines analytical method validation as establishing that a method's performance characteristics meet requirements for its intended purpose through laboratory studies. The key steps of validation include specificity, linearity, accuracy, precision, range, detection/quantitation limits, and robustness. Validation ensures testing methods are suitable and reliable for their intended use in pharmaceutical quality control.
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This document summarizes the ICH Q2 R1 Guideline on validation of analytical procedures. It discusses the objective of validation, which is to demonstrate that an analytical procedure is suitable for its intended purpose. It outlines the types of analytical procedures that should be validated, including identification tests, quantitative impurity tests, limit tests for impurities, and assay procedures. It also describes the key validation characteristics that should be tested, such as specificity, accuracy, precision, detection limit, quantitation limit, linearity, range, robustness, and system suitability. The document provides details on these validation parameters and recommends the type of data that should be collected for each parameter. It also discusses related topics like method verification versus validation and re
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The document summarizes the ICH Q2 R1 guideline on the validation of analytical procedures. It discusses the objective of validation, which is to demonstrate that an analytical procedure is suitable for its intended purpose. It describes the types of analytical procedures that should be validated, including identification tests, quantitative impurity tests, limit tests for impurities, and assay procedures. It then goes into detail describing the validation parameters that should be tested, including specificity, accuracy, precision, detection limit, quantitation limit, linearity, range, robustness, and system suitability. The document provides information on how to validate both compendial and non-compendial analytical procedures, as well as the concept of verification for compendial methods
Seminar on introduction to validation
This presentation include general introduction to validation of analytical method . analytical method validation include following points such as :
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The document defines method validation and discusses its importance for developing confidence in analytical methods and meeting regulatory requirements. It describes when validation is necessary, such as for compendial or non-compendial methods. Key validation characteristics are discussed, including accuracy, precision, specificity, linearity, range, detection and quantification limits, and robustness. The document provides guidance on testing for these characteristics and establishing acceptance criteria to ensure analytical methods are suitable for their intended purposes.
HPLC validation.ppt
This document discusses method validation. It defines method validation as proving an analytical method is suitable for its intended purpose. Validation ensures consistent, reliable and accurate data. Methods must be validated when parameters have changed or the method scope has expanded. Validation includes tests for accuracy, precision, specificity, linearity, range, limit of detection, limit of quantification and robustness. The document outlines validation procedures and acceptance criteria for different analytical methods and techniques.
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The document discusses various aspects of analytical method validation including the key parameters to evaluate, strategies for validation, documentation requirements, and regulatory guidelines. It defines method validation as confirming the suitability of an analytical procedure for its intended use. Key parameters discussed include accuracy, precision, specificity, range, linearity, limits of detection and quantitation, ruggedness, and robustness. Validation involves experimental testing, documentation in a report, and approval. Methods must be validated before use and revalidated if changed. The document provides detailed guidance on conducting and documenting the method validation process.
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Seminar by prakash on validation
- 1. A S E M I N A R O N V A L I D A T I O N O F A N A L Y T I C A L M E T H O D A S P E R I C H G U I D E L I N E S P R E S E N T E D B Y P R A K A S H G U P T A I S T S E M D E P A R T M E N T O F P H A R M A C E U T I C A L A N A L Y S I S S U B M I T T E D T O D R C S R KARNATAKA COLLEGE OF PHARMACY
- 2. VALIDATION OF ANALYTICAL METHOD AS PER ICH GUIDELINES
- 3. 1.Food and drug administration (FDA): It is a establishing documentation evidence, which provides a high degree of assurance that specific process, will consistently produce a product meeting its predetermined specifications and quality attributes. 2. World health organization (WHO): Action of providing that any procedure, process, equipment, material, activity, or system actually leads to the expected results.
- 4. 3. European committee (EC): Action of providing in accordance with the principles of good manufacturing practice, that any process, equipment material, activity or system actually leads to the expected results. In brief validation is a key process for effective quality assurance.
- 5. OBJECTIVE OF VALIDATION The primary objective of validation is to form a basis for written procedures for production and process control which are designed to identity strength quality and purity Quality, safety, and efficacy must be designed and build into the products. Each step of the manufacturing process must be controlled to maximize the probability that the finished products meet all quality and design specifications.
- 6. BENEFITS Quality, patient satisfaction, it has been built into the product. In understanding equipment systems, process improvement, technology transfer, related product validation. Rapid failure investigations, increased employee awareness.
- 7. TYPES OF VALIDATION 1. Product validation 2. Process validation 3. Personnel validation 4. Cleaning validation 5. Method validation
- 8. METHOD VALIDATION Definition: Method validation is the process to confirm that analytical procedure employed for specific test is suitable for its intended use. OR It is an act of proving that any procedure, process, equipment, material, activity of system.
- 9. According to ICH typical analytical performance characteristics that should be considered in the validation of the types of methods are 1. Specificity 2. Linearity 3. Range 4. Accuracy 5. Precision 6. Detection limit 7. Quantitation limit 8. Robustness 9. Ruggedness
- 10. • SPECIFICITY – Identification- suitable identification tests should be able to discriminate between compounds of closely related structures. Ex- IR spectrum , for chromatographic procedures representative chromatograms should be used to demonstrate specificity. – Assay and Impurity tests is done to 1. Discrimination of analytes where impurities are available. 2. Discrimination of analytes where impurities are not available.
- 11. • Figure 4. Examples of pure and impure HPLC peaks. The chromatographic signal does not indicate any impurity in either peak. Spectral evaluation, however, identifies the peak on the left as impure.
- 12. LINEARITY: For the establishment of linearity, a minimum of 5 concentrations are recommended. linearity should be evaluated by visual inspection of a plot of signals as a function of analyte concentration and finally evaluated by statistical methods. RANGE: The specified range is normally derived from linearity studies and depends on the intended application of the procedure. It is established by conforming that the analytical procedure provides an acceptable degree of linearity, accuracy, and precision.
- 13. ACCURACY: Accuracy is calculated as the percentage of recovery by the assay of the known added amount of analyte in the sample or as the difference between the mean and the accepted true value, together with confidence intervals. The ICH documents recommended that accuracy should be assed using a minimum of nine determinations over a minimum of three concentrations levels covering the specified range • Assay: 1. Drug substance 2. Drug product • Impurities • Recommended data
- 14. PRECISION: It is usually expressed as a variance standard deviation or coefficient of variation of a series of measurements. Precision can be expressed as Repeatability-under same operating conditions Intermediate precision-within laboratory variations Reproducibility-in different laboratories Recommended data QUANTITATION LIMIT: Expressed as concentration of the analyte Lowest amount of analyte in a sample that can be determined with precision and accuracy under same experimental conditions.
- 15. • Approaches listed below may be acceptable: • 1.Based on visual evaluation • 2.Based on signal to noise • 3.Based on the standard deviation of the response and slope: • The quantitation limit (QL) may be expressed as: • (QL) = 10 × standard deviation of the response • slope of the calibration curve
- 16. Typical variations affecting a method’s reproducibility Instrument • batches of accessories e.g. chrom. Columns • Operators • Sample matrices • Concentration • Batches of material, e.g., reagents • Environmental conditions, e.g., temperature • Laboratory
- 17. ROBUSTNESS • It should show the reliability of analysis with respect to delibrate variations in method parameters Examples of variation- – Extraction time – Temperature RUGGEDNESS • Measurement of reproducibility of Test results under the variation in condition normally expected from laboratory to laboratory
- 18. • DETECTION OF LIMIT: – Based on Visual Evaluation – Based on signal to noise ratio – Based on standard deviation of the response and the slope DL=3.3∫S ∫=the standard deviation of the response S=slope of the calibration curve ∫ can be calculated by – Standard deviation of the blank – Calibration curve
- 19. REFERENCES -Mark H. 2003. Application Of Improved Procedure For Testing Linearity Of Analutical Method To Pharmaceutical Analsysis, J. Pham and Biomed Anl. 33, 7-20. -WWW.GOOGLE.COM.